تفاعل #52247

ord-744b6f7830e74138ba8d3a0fa822c2b4

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىpurged with nitrogen
  2. 2
    workup.ADDITIONOne drop of dibutyl tin dilaurate was added to the solution
  3. 3
    workup.STIRRINGto stir overnight
  4. 4
    أخرىa white precipitate was obtained
  5. 5
    أخرىafter solvent removal m.p. 105-112° C. (40.5 g, 100%)

الإجراء التجريبي

Hydroxy ethylmaleimide (10 g, 0.141 mol) was dissolved in acetone and purged with nitrogen while stirring in an ice bath. One drop of dibutyl tin dilaurate was added to the solution. The isophorone diisocyanate (30.5 g, 0.141 mol) was added dropwise over 2-3 hours. The solution was allowed to stir overnight and a white precipitate was obtained after solvent removal m.p. 105-112° C. (40.5 g, 100%). 1H-NMR (D6-DMSO, δ, ppm): 3.63-3.58 (2H, —NCH2—), 4.08-4.03 (2H, —CH2O—, t), 7.03 (2H, —CH═CH—, s). 13C-NMR (D6-DMSO, δ, ppm): 134.5 (2C, —CH═CH—), 154.9 (2C, NHC═O), (170.7 (2C, —NC═O).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06855745B2uspto-grants-2005_02